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Agilent Technologies PL-GPC 220 Скачать руководство пользователя страница 93

PL-GPC 220 User Manual

93

Maintenance

7

Differential Refractive Index Detector

Differential Refractive Index Detector 

The differential refractive index detector (DRI) is designed specifically for 
high temperature chromatography giving an excellent signal to noise ratio 
even at temperatures up to 220 °C. The light source and detectors are both 
external to the oven and only the optical bench is heated and maintained at 
the oven temperature.

In normal operation, very few problems are usual encountered with the DRI, 
since the tubing and cell are continually washed with solvent. However, to 
prevent contamination of the cell during the times when the system is not 
operated, we recommend that the system is flushed and stored in acetone or 
methanol. If the cell does become dirty, which will be manifested by a 
reduction in the chromatography performance and typically small peaks, we 
recommend the following sequence of maintenance to be carried out in order:

1

Purging the DRI Cell

2

Flushing the DRI Cell with a Cleaning Agent

3

Removal of the Cell and Replacement of Seals

Содержание PL-GPC 220

Страница 1: ...Agilent Technologies Agilent PL GPC 220 Integrated HT GPC SEC System User Manual PL GPC 220 User Manual...

Страница 2: ...ms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with...

Страница 3: ...tions 3 Unpacking the Instrument This chapter gives information on how to unpack your PL GPC 220 4 Using the Module This chapter provides information on how to set up the instrument for an analysis an...

Страница 4: ...4 PL GPC 220 User Manual In This Guide 8 Parts for Maintenance This chapter provides information on parts for maintenance 9 Appendix This chapter provides addition information on safety legal and web...

Страница 5: ...Unpacking the Instrument 25 Unpacking the Instrument 26 4 Using the Module 29 The Graphical User Interface 30 Setting Up the PL GPC 220 45 Running Samples on the PL GPC 220 53 5 Troubleshooting and Di...

Страница 6: ...t 90 Back Pressure Regulator BPR 91 Differential Refractive Index Detector 93 Autosampler 97 8 Parts for Maintenance 103 Parts List 104 Pump Spares 105 9 Appendix 107 General Safety Information 108 Th...

Страница 7: ...GPC 220 Introduction 8 System Description and General Operation 9 Instrument Overview 9 Solvent Module 11 Column Oven 13 PL GPC 220 Autosampler 15 Injection Sequence 17 This chapter gives an instrume...

Страница 8: ...arousel high sensitivity refractive index detector and a reliable isocratic solvent delivery system housed uniquely in a temperature controlled enclosure The open architecture of the column oven enabl...

Страница 9: ...L GPC 220 1 System Description and General Operation System Description and General Operation Instrument Overview Figure 2 Overview modules 1 Control drawer 2 Autosampler 3 Main oven module 4 Solvent...

Страница 10: ...ral Operation Figure 3 Overview display and control elements 1 Power switches 2 Oven over temperature display and control 3 Autosampler over temperature display and control 4 Temperature and RI displa...

Страница 11: ...is then circulated across the pump head and degasser and ventilated from the rear of the unit A vapor sensor located at the rear of the bottom section of the solvent module samples the air before it...

Страница 12: ...iner run too low or the waste container get too full No action by the instrument will take place at this point and therefore it is advisable to check the levels in the solvent vessels daily and to set...

Страница 13: ...1 System Description and General Operation Column Oven Figure 6 Standard Oven Configuration 1 Oven Fan with Heaters 2 Temperature Sensors 3 Differential Refractive Index Detector 4 Sample Needle Assem...

Страница 14: ...emperature within the oven is controlled by eight active heaters 3 are built into the base of the oven and 4 in the oven lid the eighth heater is mounted directly in front of the fan and it is this he...

Страница 15: ...d as a waste container should an injection sequence malfunction In this case the contents of the loop and injection system will be emptied into this index vial to circumvent blockage due to precipitat...

Страница 16: ...anual 1 Introduction to PL GPC 220 System Description and General Operation Figure 8 Temperature controlled zones in the carousel di odcZ LVgb odcZ c_ZXi dc ed ci c_ZXi dc ed ci K Va edh i dc 8VgdjhZa...

Страница 17: ...Default condition prior to injection Injection valve in the Inject position Vial in carousel Syringe at mid point 2 Sample loaded Valve switched to load position Vial lifted to needle Syringe sucks 8...

Страница 18: ...r Manual 1 Introduction to PL GPC 220 System Description and General Operation 3 Sample injected Sample injected Excess sample from overflow loop returned to the vial Vial returned to the carousel di...

Страница 19: ...Technologies 2 Site Requirements and Specifications Site Requirements 20 Physical Specifications 23 Performance Specifications 24 This chapter provides information on environmental requirements physic...

Страница 20: ...ed the main power leads are provided with NEMA 15 type plugs The mains supply should be fitted with an RCCB Residual Current operated Circuit Breaker WARNING Hazard of electrical shock or damage of yo...

Страница 21: ...t circuit Never operate your instrumentation from a power outlet that has no ground connection Never use a power cord other than the Agilent Technologies power cord designed for your region WARNING Us...

Страница 22: ...direct sunlight Extraction Requirements The instrument is equipped with two fan forced exhausts 4 in diameter at the rear of each module which must be routed to a fume extraction system or vented int...

Страница 23: ...tion 3300 VA 2310 W 7900 BTU Line frequency 50 or 60 Hz 5 Size width depth height 1400 mm x 560 mm x 630 mm Packaged Size width depth height 930 mm x 760 mm x 860 mm Two boxes Weight 180 kg 396 lbs Am...

Страница 24: ...ance The values quoted have been calculated from analyses performed in THF at 40 C and in TCB at 160 C 0 07 RSD or 0 02 min SD whatever is greater based on retention time at constant room temperature...

Страница 25: ...25 PL GPC 220 User Manual Agilent Technologies 3 Unpacking the Instrument Unpacking the Instrument 26 This chapter gives information on how to unpack your PL GPC 220...

Страница 26: ...our service representative that the instrument may have been damaged during shipment CAUTION Defective on arrival problems If there are signs of damage please do not attempt to install the module Insp...

Страница 27: ...ons of foam packaging surrounding the unit one at each side one piece at the front and two small sections behind the unit The wires are tucked down between the two foam sections at the back Tools requ...

Страница 28: ...e instrument down to the sub platform above the main pallet 5 Cut the plastic bands to enable the unit to be lifted free from the pallet The unit can now be lifted clear of the pallet 6 Position the i...

Страница 29: ...rd 42 Time Estimator 43 System Monitor 44 Data Acquisition 44 Setting Up the PL GPC 220 45 Starting the Instrument 45 Introducing Solvent to the PL GPC 220 47 Running the PL GPC 220 49 Changing Column...

Страница 30: ...s a comprehensive monitoring system The instrument status can be rapidly assessed for each of the instrument s modules Figure 9 Graphical User Interface NOTE Onscreen help accessed directly from the s...

Страница 31: ...th the graphical representation of the instrument also shown on the interface The pump is coded blue the oven red the refractometer green and the autosampler turquoise For each of the controlled modul...

Страница 32: ...al User Interface The Toolbar The Toolbar contains the following icons K Zl ggdg Ad h 9 heaVn gVe XVa Ad h K Zl Ad h HVkZ Ad Hide Ad c HiVgi Ad c BZi dY Y idg B c b oZ BVm b oZ Ad c 9 Vad h HnhiZb Bdc...

Страница 33: ...ow rate is typically at 1 0 mL min the carousel heaters are on and the instrument is ready to run samples Following boot up the instrument will typically default to the STANDBY mode unless the instrum...

Страница 34: ...he parameters set up in autosampler configuration screen Inject this button is used to manually change the injection valve position see Injection Sequence on page 17 for the description of positions T...

Страница 35: ...needles of the dials using the up or down arrows or just simply typing the required values in the edit boxes To action a change made to the configuration the values as displayed in the configuration...

Страница 36: ...r using the up and down arrows adjacent to the Edit box Heat Rate is the rate at which the oven will heat to the set temperature To prevent excessive over shoot of the set temperature and prolonged st...

Страница 37: ...e purge valve will remain open following a manual or automatic purge command The Settle Time is the time allowed in seconds following a purge that the system waits before the autozero command is actio...

Страница 38: ...Zone and the dark blue arc the Warm Zone Hot Zone Temperature of the samples in the Hot Zone measured at vial position 1 This zone spans the injection point and the area of the carousel that is magnet...

Страница 39: ...220 Viscometer is installed in parallel then the times shown in parentheses should be used to allow the viscometer break through peak to elute before the injection of the next sample 1 column 12 min...

Страница 40: ...change any of the settings simply highlight the parameter you wish to change and type in the new value Some of the entries require a T true or F false indicating the status To save a method click on...

Страница 41: ...system will only allow a user to view the instrument control parameters and downloading any changes to these parameters will be impossible Security The Security dialog enables and disables access righ...

Страница 42: ...this box If the box is not checked then all methods are disabled and can not be used to change the instrument configuration Use the up and down arrows to select the method s to enable The Security op...

Страница 43: ...his is set correctly Check the Start Autosampler box to enable a timed A S start The Refresh button will update the finish details based on the programmed A S set up Enter the Start Day and Start Time...

Страница 44: ...data acquisition package but can be program to run a Windows based executable For convenience three data acquisition packages have been pre programmed PL Caliber TriSEC and Precision Acquire Before s...

Страница 45: ...ss the instrument will perform the following tests Test the buzzer Initialize the pump Initialize the oven Initialize the autosampler Find zero vial Raise vial into the oven Purge the syringe Lower th...

Страница 46: ...GPC 220 6 Flush the entire system with the solvent required See Introducing Solvent to the PL GPC 220 on page 47 NOTE When changing between two immiscible solvents intermediary solvent s should be use...

Страница 47: ...system and adjust the Idle flow rate to 1 0 mL min 6 Close the purge valve on the pump head and again manually turn on the pump to flush solvent through the remainder of the instrument 7 Flush the sy...

Страница 48: ...r pressure transducers is required see the G7821A PL GPC 220 Viscometer manual 10 Once the system is totally flushed into the desired chromatography solvent a Turn off the pump b Close the DRI purge v...

Страница 49: ...there are no leaks from any connections 5 Stop the flow and close both the inner and the outer oven lids 6 Put the instrument into RUN mode Wait for the oven to stabilize at the Run temperature and R...

Страница 50: ...ply replace the old columns with the new columns OR If a column solvent transfer is required carry this out according to the manufacturer s instructions 5 Manually start the flow to check for leaks En...

Страница 51: ...E mode and let the oven cool Only continue if oven is at 40 C 3 Put the instrument into STANDBY mode and open the oven lids 4 Remove the columns from the system and replace with a barrel connector 5 R...

Страница 52: ...n and the Idle temperature to 40 C 2 Put the instrument into IDLE mode and let the oven cool Only continue if oven is at 40 C 3 Put the instrument into STANDBY mode and open the oven lids 4 Replace th...

Страница 53: ...tings 8 Set the Run time typically the same as the data collection time 9 Click the Send button to update the instrument with the new autosampler settings 10 Adjust the autosampler over temperature cu...

Страница 54: ...vials 5 On the autosampler area of the Control software click the Autosampler Offline button This will now change to Autosampler Online and the sequence will begin You can follow the status of the run...

Страница 55: ...tics 56 General Troubleshooting Guide 58 Boot Up Problems 58 Autosampler Problems 59 RI Problems 59 Oven Temperature Control Problems 60 Solvent Module Problems 60 Pump Problems 60 Chromatography Prob...

Страница 56: ...s while operating the instrument a new diagnostic screen is now available from the Tools Utility menu The diagnostic utility consists of three tabbed views AS General Status displays the autosampler s...

Страница 57: ...PL GPC 220 User Manual 57 Troubleshooting and Diagnostics 5 Diagnostics Other Modules Status displays the other instrument functions Figure 14 Other Module Status...

Страница 58: ...of the PL GPC 220 Control drawer Injection valve failure Check that the Link cables on the rear of the Control drawer are connected correctly If problem persists please contact your local Agilent serv...

Страница 59: ...observing the rotation of ventilation fans in the baseplate Autosampler Problems Please contact your local Agilent service representative RI Problems Fails to autozero correctly Purge the RI thoroughl...

Страница 60: ...ntative Check that the oven lid is fully closed and seals properly Check that the power line voltage is not below 200 V Check that the ambient temperature above 10 C Ensure that the stability of power...

Страница 61: ...s if necessary The pump pressure is continually monitored when the Logging is turned on and the pressure history can viewed in the log table or plotted graphically see the LOG MENU in the graphical us...

Страница 62: ...62 PL GPC 220 User Manual 5 Troubleshooting and Diagnostics General Troubleshooting Guide Mirrored peaks Ensure that the purge valve is closed Inspect the RI cell for cracks particularly in partition...

Страница 63: ...er Manual Agilent Technologies 6 Error Information Errors 64 This chapter describes the meaning of error messages and provides information on probable causes and suggested actions how to recover from...

Страница 64: ...g the error indicator is flashed red and the beeper is sounded Depending on the severity of the error following a short time delay the instrument steps in to render the system safe Details of the erro...

Страница 65: ...and not initializing 50 s 10 s 5 Flash Red YES STBY PUMP COMMS The pump is no longer responding No serial responsefrom the pump 3 s 1 s 3 Flash Red YES STBY Oven TEMPERATURE Oven temperature has beco...

Страница 66: ...d failed responsefrom autosampler 0 Flash Red NO MOVE Failed to move carousel correctly 3 Flash Red NO VIAL LOWER Failed to lower vial from the oven 0 Flash Red NO VIAL LIFT Failed to lift vial from t...

Страница 67: ...s 3 Flash Red NO no command success response variable variable 0 Flash Red NO Solvent SOLVENT LEVEL Solvent level low or waste level high I O state change Flash Red NO SOLV VAP Vapor sensor and or ove...

Страница 68: ...68 PL GPC 220 User Manual 6 Error Information Errors...

Страница 69: ...Test 84 Testing Solvent Level Sensors 86 Testing Oven Door Interlock 88 Laser Interlock Switch 89 Degasser Test 90 Back Pressure Regulator BPR 91 Replace the Back Pressure Regulator BPR 91 Differenti...

Страница 70: ...o inspect the system periodically The instrument is designed to be a low maintenance instrument and does not generally require regular service For your convencience an annual inspection is offered as...

Страница 71: ...boratory practice The volume of substances should be reduced to the minimum required for the analysis Do not operate the instrument in an explosive atmosphere WARNING Electric shock Repair work at the...

Страница 72: ...sture enters the instrument Do not attempt to clean any connectors WARNING Personal injury or damage to the product Agilent is not responsible for any damages caused in whole or in part by improper us...

Страница 73: ...ith deionized water 4 Wipe down the exterior of the instrument 5 Allow the instrument to dry off completely before reconnecting power WARNING Liquid dripping into the electronic compartment of your in...

Страница 74: ...ssible correct the source of the leak 3 Inspect cabling parts and surfaces to determine whether or not any damage has occurred 4 Allow the the instrument to dry completely before reconnecting power 5...

Страница 75: ...er temperature protection systems to eliminate potential hazards due to failure of their respective temperature controllers The trip points of the oven and autosampler protection can be adjusted by th...

Страница 76: ...t and press the reset button to silence the alarm This concludes the oven over temperature protection system test Preparations This test can be carried out at any operating temperature above 40 C If t...

Страница 77: ...ow the over temperature set point before rising quickly 6 If the initial value shown is close to the warm zone set point then the protection system is not functioning correctly OR Once warm zone cooli...

Страница 78: ...initial value on the over temperature display while the reset button is held This indicates the higher of the two zone temperatures which should initially be at or below the over temperature set poin...

Страница 79: ...ay be necessary to remove solvent and waste bottles from the solvent module compartment to clear enough space 1 Switch ON the PL GPC 220 oven unit and solvent module and set the instrument to IDLE 2 S...

Страница 80: ...hot water for a few minutes and check the temperature of the heat sink again This should now be noticeably cooler 8 If the alarm condition does not occur or the heatsink does not cool down then switch...

Страница 81: ...PL GPC 220 User Manual 81 Maintenance 7 Testing Vapor Sensors Testing Vapor Sensors The vapor sensors are tested by simulating a solvent leak or spillage in the following modules Oven Solvent module...

Страница 82: ...notification will appear on the Control software 4 Open the solvent module front flap and check that the pump and degasser module are powered down 5 If the alarm condition does not occur or if the pu...

Страница 83: ...Remove the paper ball from the solvent module and dispose of it appropriately 7 Close the front flap again and wait a minute or so until the solvent module alarm ceases 8 Clear the error on the Contro...

Страница 84: ...STANDBY mode click OK to confirm 5 Open the outer and inner oven lids and place the paper on the floor of the oven near the RI far away from the spiral heater and fan see Oven Vapor Sensor Test on pag...

Страница 85: ...r if the pump flow has not stopped after three minutes then switch off and disconnect the power cords from both units 10 Open the oven and remove the paper Dispose of it appropriately 11 Leave the ove...

Страница 86: ...ng Solvent Level Sensors If your PL GPC 220 solvent module is fitted with steel solvent tanks a pair of liquid level sensing float switches will have been provided These can be tested after removing t...

Страница 87: ...float switch waste level high OR Test the low solvent level by lowering the solvent float switch solvent level low Both of these two abnormal conditions should produce an audible solvent module alarm...

Страница 88: ...nstrument is running 1 Set the instrument to IDLE or RUN mode 2 Open the outer oven door An audible alarm should sound immediately and an error notification should be displayed by the Control software...

Страница 89: ...he oven door interlock is a safety interlock switch which will turn off the laser in the light scattering detector when installed when the oven door is opened 1 Check the connection of cable from the...

Страница 90: ...of the the pump unit built into the solvent delivery module and is designed to remove dissolved gas from the solvent The dissolved gas is removed from the solvent through a membrane thin wall PTFE tub...

Страница 91: ...during the purge cycle To ensure optimum performance of the chromatography columns it is important to maintain flow through the columns at all times when operating at high temperature The purge valve...

Страница 92: ...k Pressure Regulator BPR 3 Fit the replacement BPR with the arrow in the direction of the flow for example from right to left 4 Turn on the flow and open the PURGE valve Check the system backpressure...

Страница 93: ...ature In normal operation very few problems are usual encountered with the DRI since the tubing and cell are continually washed with solvent However to prevent contamination of the cell during the tim...

Страница 94: ...low the system to purge at 2 0 mL min for 15 min during which time the baseline can be monitored and should give a flat noise free baseline If the baseline is off scale press the Autozero button on th...

Страница 95: ...om the conventional arrangement Figure 17 on page 96 to sample and reference in series Figure 18 on page 96 When Purging the reference side of the DRI cell does not cure the baseline noise or lack of...

Страница 96: ...l Refractive Index Detector Figure 17 Conventional Plumbing Figure 18 Sample and Reference in Series for Continuous Flushing Ejg Z 8dajbc LVhiZ A cZ G H Id gZ ZgZcXZ d G WadX Ejg Z 8dajbc LVhiZ A cZ 7...

Страница 97: ...Maintenance 7 Autosampler Autosampler To ensure optimum performance of the autosampler system it is recommended that the following important maintenance procedures be performed every 3 6 months depen...

Страница 98: ...the syringe from its mounting Disconnect it from the Luer lock needle assembly 3 If the syringe is contaminated with solvent wash it out with acetone and dry 4 Place a couple of drops of silicone oil...

Страница 99: ...e top section of the panel front and up and disconnect the earth cable from the panel b Unscrew the clamping screw located at the rear and bottom of the lower panel and the small x head screw located...

Страница 100: ...rs 2 With a piece of tissue paper moistened with acetone wipe clean the entire track that the vial holders sit on 3 Using a cotton bud Q tip sprinkle a small amount of graphite powder over the track 4...

Страница 101: ...tating with an 11 mm wrench 4 Remove the interconnecting capillary tubing and push to one side to ease access to the needle 5 Unscrew the two M3 stainless steel socket cap head screws on the side and...

Страница 102: ...al 7 Maintenance Autosampler 10 Holding the needle assembly firmly in position tighten the two M3 stainless steel socket cap screws 11 Reconnect the capillary tubing 12 Reconnect the power lead s and...

Страница 103: ...103 PL GPC 220 User Manual Agilent Technologies 8 Parts for Maintenance Parts List 104 Pump Spares 105 This chapter provides information on parts for maintenance...

Страница 104: ...Parts List Parts List p n Description PL0870 6110 Solvent reservoir filter PL0800 0003 Injection valve rotor seal PL1 23926 Vial locator solenoid and plunger assembly PL4 32434 Replacement Inline fil...

Страница 105: ...20 Cartridge for active inlet valve 600 bar G1312 60022 Outlet ball valve 5067 4728 Seal cap 5063 6586 2x Sapphire piston 0905 1175 2x Wash seal PTFE 01018 22707 PTFE frits pack of 5 5063 6589 Standar...

Страница 106: ...106 PL GPC 220 User Manual 8 Parts for Maintenance Pump Spares...

Страница 107: ...ymbols 108 General Safety Information 109 Safety Standards 109 Operation 109 Precautions 111 The Waste Electrical and Electronic Equipment Directive 113 Radio Interference 114 Sound Emission 115 Agile...

Страница 108: ...gerous voltages Indicates a protected ground terminal The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up WARNING A WARNING alerts...

Страница 109: ...ing must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it mu...

Страница 110: ...with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard...

Страница 111: ...f using methods not recommended by Agilent Technologies check with Agilent Technologies that the method will not damage the instrument Perform periodic leak checks on all wetted components tubing and...

Страница 112: ...surges by filtering the incoming supply CAUTION Solvent vapors Liberal use of organic solvents in close proximity to the instrument may activate the vapor sensors causing the instrument to shutdown E...

Страница 113: ...nces starting with 13 August 2005 NOTE This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard this electrical electronic pr...

Страница 114: ...protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for...

Страница 115: ...statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position 70 dB Sound Pressure...

Страница 116: ...Appendix Agilent Technologies on Internet Agilent Technologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Sele...

Страница 117: ...ock switch check 89 M methods editor 40 O oven door interlock test 88 overtemperature protection test autosampler 77 oven 76 solvent module 79 P packaging damaged 26 password changing 42 performance s...

Страница 118: ...118 PL GPC 220 User Manual Index U unpacking 27 V vapor sensor test solvent module 84 82 W waste electrical and electronic equipment 113 WEEE directive 113...

Страница 119: ......

Страница 120: ...hnologies In This Book This manual contains information on the Agilent PL GPC 220 Integrated HT GPC SEC System G7820A The manual describes the following General information Introduction Site requireme...

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